Spin-crossover behavior of neutral iron(iii) complexes with salicylaldehyde thio-, seleno- and semicarbazone ligands: experiment and theoretical analysis.
Spitsyna, Nataliya G.; Blagov, Maxim A.; Lazarenko, Vladimir A.; Zorina, Leokadiya V.; Vasiliev, Alexander N.; Krapivin, Vladimir B.; Svetogorov, Roman D.; Maximova, Olga V.; Simonov, Sergey V.; Yagubskii, Eduard B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9328–9336; doi:10.1039/c9dt01404g

data_7700052
_publ_section_title
;
 Spin-crossover behavior of neutral iron(iii) complexes with
 salicylaldehyde thio-, seleno- and semicarbazone ligands: experiment and
 theoretical analysis.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9328
_journal_page_last               9336
_journal_paper_doi               10.1039/c9dt01404g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C16 H15 Fe N6 O4, 3(H2 O)'
_chemical_formula_sum            'C16 H21 Fe N6 O7'
_chemical_formula_weight         465.24
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-13 deposited with the CCDC.    2019-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.77(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.587(4)
_cell_length_b                   12.556(3)
_cell_length_c                   9.0534(18)
_cell_measurement_reflns_used    700
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      2.25
_cell_measurement_theta_min      30.8
_cell_volume                     1994.9(8)
_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      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       /f
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80246
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21114
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.853
_diffrn_reflns_theta_min         2.252
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.031(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4319
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0631
_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^)+(0.1205P)^2^+1.0317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3812
_reflns_number_total             4319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01404g2.cif
_cod_data_source_block           fe3
_cod_depositor_comments          'Adding full bibliography for 7700052.cif.'
_cod_original_cell_volume        1994.8(7)
_cod_database_code               7700052
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.877
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H5A-O5
 0.84 with sigma of 0.02
 H5B-O5
 0.84 with sigma of 0.02
 H6C_$3-O6_$3
 0.84 with sigma of 0.02
 H6D_$3-O6_$3
 0.84 with sigma of 0.02
 H6C-O6
 0.84 with sigma of 0.02
 H6D-O6
 0.84 with sigma of 0.02
 H7A-O7
 0.84 with sigma of 0.02
 H7B-O7
 0.84 with sigma of 0.02
 N6-H6B \\sim N6-H6A
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
  C14(H14)
;
_shelx_res_checksum              34404
_olex2_submission_special_instructions 'No special instructions were received'