Hysteretic thermal spin-crossover in heteroleptic Fe(ii) complexes using alkyl chain substituted 2,2′-dipyridylamine ligands
Geoghegan, Blaise L.; Phonsri, Wasinee; Horton, Peter N.; Orton, James B.; Coles, Simon J.; Murray, Keith S.; Cragg, Peter J.; Dymond, Marcus K.; Gass, Ian A.; Dalton Transactions  (2019) –; doi:10.1039/C9DT03412A

data_7701947
_publ_section_title
;
 Hysteretic thermal spin-crossover in heteroleptic Fe(ii) complexes using
 alkyl chain substituted 2,2&#x2032;-dipyridylamine ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03412A
_journal_year                    2019
_chemical_formula_moiety         'C42 H54 Fe N8 O2 S2'
_chemical_formula_sum            'C42 H54 Fe N8 O2 S2'
_chemical_formula_weight         822.90
_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     direct
_audit_block_doi                 10.5517/ccdc.csd.cc23clnr
_audit_creation_date             2019-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-16 deposited with the CCDC.	2019-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.966(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9129(9)
_cell_length_b                   8.2544(3)
_cell_length_c                   17.5843(9)
_cell_measurement_reflns_used    5384
_cell_measurement_temperature    105
_cell_measurement_theta_max      30.1470
_cell_measurement_theta_min      2.5560
_cell_volume                     2093.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      105
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -24.00  28.00   0.50    6.00    --    5.00  57.00-180.00  104
  2  \w    -17.00  51.00   0.50    6.00    --   -6.30  60.00  30.00  136
  3  \w    -93.00  10.00   0.50    6.00    --   -6.30 -19.00  60.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0487693000
_diffrn_orient_matrix_UB_12      -0.0005176000
_diffrn_orient_matrix_UB_13      0.0237745000
_diffrn_orient_matrix_UB_21      -0.0018159000
_diffrn_orient_matrix_UB_22      0.0811804000
_diffrn_orient_matrix_UB_23      0.0124981000
_diffrn_orient_matrix_UB_31      -0.0060060000
_diffrn_orient_matrix_UB_32      -0.0281766000
_diffrn_orient_matrix_UB_33      0.0354715000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15148
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       'cut lath'
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0400P)^2^+1.1892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4156
_reflns_number_total             4816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03412a2.cif
_cod_data_source_block           1C10105K
_cod_database_code               7701947
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C84 H108 N16 O4 S4 Fe2'
_chemical_oxdiff_usercomment     BGP901_140K
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.907
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_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 1.505
_oxdiff_exptl_absorpt_empirical_full_min 0.619