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_7711708
_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         'C44 H40 Cl2 Fe'
_chemical_formula_sum            'C44 H40 Cl2 Fe'
_chemical_formula_weight         695.51
_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             2021-04-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-07 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.9930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   22.1189(2)
_cell_length_b                   19.6861(2)
_cell_length_c                   24.7347(2)
_cell_measurement_reflns_used    41546
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.5010
_cell_measurement_theta_min      3.9420
_cell_volume                     10711.49(17)
_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 2014/5 (Sheldrick, 2014)'
_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 5.2349
_diffrn_detector_type            'Agilent Diffraction Atlas S2 detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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    -94.00  -2.00   1.00    7.50    --  -38.50 125.00-120.00   92
  2  \w      6.00 122.00   1.00    7.50    --   43.08  19.00 -30.00  116
  3  \w     16.00 113.00   1.00    7.50    --   43.08  57.00  30.00   97
  4  \w     23.00 109.00   1.00   30.00    --  104.50 -94.00 -30.00   86
  5  \w     30.00  91.00   1.00   30.00    --  104.50 -30.00 150.00   61
  6  \w     33.00 122.00   1.00   30.00    --  104.50-125.00 -90.00   89
  7  \w     30.00  91.00   1.00   30.00    --  104.50 -30.00  60.00   61
  8  \w     33.00  98.00   1.00   30.00    --  104.50 -45.00-180.00   65
  9  \w     73.00 176.00   1.00   30.00    --  104.50 125.00-180.00  103
 10  \w     80.00 176.00   1.00   30.00    --  104.50  45.00-180.00   96
 11  \w     31.00 136.00   1.00   30.00    --  104.50 -77.00  90.00  105
 12  \w     16.00 113.00   1.00    7.50    --   43.08  57.00 150.00   97
 13  \w      2.00  98.00   1.00    7.50    --   43.08-125.00 150.00   96
 14  \w     12.00 117.00   1.00    7.50    --   43.08  77.00-150.00  105
 15  \w     59.00  94.00   1.00   30.00    --  104.50  15.00 -30.00   35
 16  \w     81.00 178.00   1.00   30.00    --  104.50  30.00  90.00   97
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Atlas 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      0.0310064000
_diffrn_orient_matrix_UB_12      0.0694880000
_diffrn_orient_matrix_UB_13      0.0106193000
_diffrn_orient_matrix_UB_21      0.0508758000
_diffrn_orient_matrix_UB_22      -0.0341674000
_diffrn_orient_matrix_UB_23      0.0378512000
_diffrn_orient_matrix_UB_31      0.0368297000
_diffrn_orient_matrix_UB_32      -0.0113454000
_diffrn_orient_matrix_UB_33      -0.0487353000
_diffrn_radiation_collimation    'focusing mirrors'
_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  0.0554
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            92429
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.959
_diffrn_reflns_theta_min         3.399
_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    4.981
_exptl_absorpt_correction_T_max  0.400
_exptl_absorpt_correction_T_min  0.158
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_recrystallization_method 'Recrystallised from hexane at -30.'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.487
_exptl_crystal_size_min          0.309
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1294
_refine_ls_number_reflns         21283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+3.7154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19286
_reflns_number_total             21283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03531f2.cif
_cod_data_source_block           kewjmc
_cod_database_code               7711708
_nottingham_internal_coll_name   KEWJMC
_nottingham_internal_coll_number 16741
_nottingham_internal_coll_client KEW/JM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '7.50, 30.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   07/12/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 09/12/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 09/12/2016
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 09/12/2016
_nottingham_internal_refinement_user pcxav1
_nottingham_internal_self_archive_date 09/12/2016
_nottingham_internal_self_validation_date 09/12/2016
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date 06/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 06/05/2022
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H40 Cl2 Fe'
_chemical_oxdiff_usercomment
'KEWJMC #16741 SN-1249 IN FOMBLIN ON A MICROMOUNT FOR AJV/DLK'
_reflns_odcompleteness_completeness 99.95
_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),
  C47(H47), C49(H49), C53(H53), C54(H54), C55(H55), C61(H61), C62(H62),
 C63(H63), C69(H69), C71(H71), C75(H75), C76(H76), C77(H77), C83(H83), C84(H84),
  C85(H85), C91(H91), C93(H93), C97(H97), C98(H98), C99(H99), C105(H105),
 C106(H106), C107(H107), C113(H113), C115(H115), C119(H119), C120(H120),
 C121(H121), C127(H127), C128(H128), C129(H129)
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), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C87(H87A,H87B,
 H87C), C88(H88A,H88B,H88C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F),
 C109(H10G,H10H,H10I), C110(H11A,H11B,H11C), C123(H12A,H12B,H12C), C124(H12D,
 H12E,H12F), C131(H13D,H13E,H13F), C132(H13G,H13H,H13I)
;
_shelx_res_checksum              81539
_shelx_hkl_checksum              48792
_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 1.534
_oxdiff_exptl_absorpt_empirical_full_min 0.654