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_7700488
_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_absolute_configuration ad
_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
_audit_creation_date             2018-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_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                   12.3433(8)
_cell_length_b                   14.3546(8)
_cell_length_c                   19.2425(14)
_cell_measurement_reflns_used    2928
_cell_measurement_temperature    123
_cell_measurement_theta_max      70.5
_cell_measurement_theta_min      6.6
_cell_volume                     3409.4(4)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
    Number of images: 24
               Slice: 20.0000 - 140.0000
         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: 30
               Slice: 20.0000 - 170.0000
         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: 31
               Slice: 21.0000 - 176.0000
         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: 32
               Slice: 22.0000 - 182.0000
         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
;
Crystal Goniometer
;
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.016906
_diffrn_orient_matrix_UB_12      -0.010153
_diffrn_orient_matrix_UB_13      0.050257
_diffrn_orient_matrix_UB_21      -0.008367
_diffrn_orient_matrix_UB_22      0.068730
_diffrn_orient_matrix_UB_23      0.006569
_diffrn_orient_matrix_UB_31      -0.078789
_diffrn_orient_matrix_UB_32      -0.005120
_diffrn_orient_matrix_UB_33      -0.011481
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1447
_diffrn_reflns_av_unetI/netI     0.1465
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_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            18081
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        50.421
_diffrn_reflns_theta_max         50.421
_diffrn_reflns_theta_min         6.598
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.346
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.091
_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    1.748
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         3505
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1137P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2225
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2318
_reflns_number_total             3505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02373a2.cif
_cod_data_source_block           pi28-lt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700487--7700489.cif.
;
_cod_database_code               7700488
_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. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C26)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) = Uanis(N1)
3.a Free rotating group:
 O6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C31(H31), C6(H6), C7(H7), C19(H19), C12(H12), C8(H8), C30(H30),
 C2(H2), C14(H14), C24(H24), C28(H28), C17(H17), C1(H1), C18(H18), C34(H34),
 C35(H35), C37(H37), C38(H38), C22(H22), C23(H23), C3(H3), C15(H15), C26(H26)
3.c Fitted hexagon refined as free rotating group:
 C33(C34,C35,C36,C37,C38)
3.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_shelx_res_checksum              12535
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'