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_7701949
_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_absolute_configuration unk
_chemical_formula_moiety         'C30 H30 Fe N8 O2 S2'
_chemical_formula_sum            'C30 H30 Fe N8 O2 S2'
_chemical_formula_weight         654.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_Int_Tables_number      33
_audit_block_doi                 10.5517/ccdc.csd.cc23clkn
_audit_creation_date             2018-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-08-16 deposited with the CCDC.	2019-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2689(10)
_cell_length_b                   8.5587(4)
_cell_length_c                   21.2446(12)
_cell_measurement_reflns_used    2872
_cell_measurement_temperature    120
_cell_measurement_theta_max      23.4610
_cell_measurement_theta_min      2.5290
_cell_volume                     3139.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.9933
_diffrn_measured_fraction_theta_max 0.9933
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1121
_diffrn_reflns_av_unetI/netI     0.1177
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27536
_diffrn_reflns_theta_full        27.5000
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.3846
_exptl_crystal_description       plate
_exptl_crystal_F_000             1362.8335
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.7309
_refine_diff_density_min         -0.8354
_refine_diff_density_rms         0.1708
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_d_res_high            0.7700
_refine_ls_d_res_low             10.6223
_refine_ls_goodness_of_fit_ref   1.0098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7154
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0098
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.3481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.987
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                4326
_reflns_number_total             7154
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9dt03412a2.cif
_cod_data_source_block           1C4120K
_cod_original_sg_symbol_Hall     ' P 2c -2n'
_cod_database_code               7701949
_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), C27(H27a,H27b), C28(H28a,H28b)
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), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C29(H29a,H29b,H29c)
;
_olex2_submission_special_instructions 'No special instructions were received'