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_7700489
_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 Fe I2 N4 O2, C7 H7 O3 S, 2(H2 O)'
_chemical_formula_sum            'C39 H31 Fe I2 N4 O7 S'
_chemical_formula_weight         1010.39
_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                   12.7045(3)
_cell_length_b                   14.1173(3)
_cell_length_c                   20.3416(14)
_cell_measurement_reflns_used    5211
_cell_measurement_temperature    103
_cell_measurement_theta_max      72.0
_cell_measurement_theta_min      7.0
_cell_volume                     3648.3(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 36
               Slice: 20.0000 - 200.0000
         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: 53.0000 - 188.0000
         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
scan:
    Number of images: 24
               Slice: 76.0000 - 196.0000
         Image width: 5.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku Spider
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.047543
_diffrn_orient_matrix_UB_12      -0.029083
_diffrn_orient_matrix_UB_13      -0.033580
_diffrn_orient_matrix_UB_21      0.001623
_diffrn_orient_matrix_UB_22      -0.060121
_diffrn_orient_matrix_UB_23      0.025976
_diffrn_orient_matrix_UB_31      -0.062711
_diffrn_orient_matrix_UB_32      -0.023605
_diffrn_orient_matrix_UB_33      -0.024786
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.1070
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17087
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        58.925
_diffrn_reflns_theta_max         58.925
_diffrn_reflns_theta_min         6.970
_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    17.621
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.695
_refine_diff_density_min         -2.059
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 1254 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.071(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         5002
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0709P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.912
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                3957
_reflns_number_total             5002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02373a2.cif
_cod_data_source_block           pi24-lt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_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               7700489
_shelx_estimated_absorpt_t_max   0.300
_shelx_estimated_absorpt_t_min   0.144
_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
C29 \\sim C28 \\sim C27 \\sim C32 \\sim C31 \\sim C30: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C16 \\sim C15 \\sim C14 \\sim C13 \\sim C12 \\sim C11: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C29) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed X: H7A(0.60614) H7B(0.4938)
 Fixed Y: H7A(0.03725) H7B(0.05494)
 Fixed Z: H7A(0.047569) H7B(0.046599)
4.a Free rotating group:
 O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C12(H12), C30(H30), C18(H18), C19(H19), C15(H15), C8(H8), C6(H6),
 C10(H10), C24(H24), C17(H17), C14(H14), C3(H3), C22(H22), C31(H31), C7(H7),
 C26(H26), C2(H2), C23(H23), C1(H1), C37(H37), C34(H34), C38(H38), C35(H35)
4.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'