Abrupt spin crossover in iron(iii) complexes with aromatic anions.
Lazaro, Sharon E.; Alkaş, Adil; Lee, Seok J.; Telfer, Shane G.; Murray, Keith S.; Phonsri, Wasinee; Harding, Phimphaka; Harding, David J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15515–15520; doi:10.1039/c9dt02373a

data_7700487
_publ_section_title
;
 Abrupt spin crossover in iron(iii) complexes with aromatic anions.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15515
_journal_page_last               15520
_journal_paper_doi               10.1039/c9dt02373a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H20 Br2 Fe N4 O2, C7 H7 O3 S, H2 O'
_chemical_formula_sum            'C39 H29 Br2 Fe N4 O6 S'
_chemical_formula_weight         897.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2019-06-05 deposited with the CCDC.    2019-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4432(3)
_cell_length_b                   14.6561(4)
_cell_length_c                   19.1005(13)
_cell_measurement_reflns_used    8805
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.6
_cell_volume                     3483.3(3)
_computing_cell_refinement       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 34
               Slice: 22.0000 - 192.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 26
               Slice: 42.0000 - 172.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 27
               Slice: 20.0000 - 155.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 34
               Slice: 23.0000 - 193.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.017985
_diffrn_orient_matrix_UB_12      -0.039011
_diffrn_orient_matrix_UB_13      -0.041325
_diffrn_orient_matrix_UB_21      -0.006619
_diffrn_orient_matrix_UB_22      -0.055817
_diffrn_orient_matrix_UB_23      0.029801
_diffrn_orient_matrix_UB_31      -0.078047
_diffrn_orient_matrix_UB_32      -0.004256
_diffrn_orient_matrix_UB_33      -0.012050
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1167
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19306
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        50.422
_diffrn_reflns_theta_max         50.422
_diffrn_reflns_theta_min         6.577
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Cu
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.190
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 756 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.499(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0773
_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^)+(0.1147P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2198
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                2414
_reflns_number_total             3616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02373a2.cif
_cod_data_source_block           pi28-rt
_cod_depositor_comments
'Adding full bibliography for 7700487--7700489.cif.'
_cod_database_code               7700487
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.479
_shelx_estimated_absorpt_t_min   0.207
_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, All O(H,H) groups
2. Restrained distances
 H6A-O5
 1.966 with sigma of 0.02
 H6B-O3_$1
 2.046 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Free rotating group:
 O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C1(H1), C2(H2), C3(H3), C28(H28), C30(H30), C31(H31),
 C12(H12), C15(H15), C14(H14), C26(H26), C10(H10), C24(H24), C23(H23), C22(H22),
  C17(H17), C18(H18), C19(H19), C38(H38), C37(H37), C35(H35), C34(H34)
4.c Fitted hexagon refined as free rotating group:
 C32(C27,C28,C29,C30,C31), C13(C12,C11,C16,C15,C14), C38(C37,C36,C35,C34,C33)
4.d Naphthalene refined as free rotating group:
 C9(C8,C7,C6,C4,C5,N1,C1,C2,C3), C25(C24,C23,C22,C20,C21,N3,C17,C18,C19)
4.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_olex2_submission_special_instructions 'No special instructions were received'