High temperature spin crossover behaviour of mononuclear bis-(thiocyanato)iron(II) complexes with judiciously designed bidentate N-donor Schiff bases with varying substituents.
Bhar, Kishalay; Guo, Wenbin; Gonidec, Mathieu; Nikhil Raj M, Venkata; Bhatt, Surabhi; Perdih, Franc; Guionneau, Philippe; Chastanet, Guillaume; Sharma, Anuj K.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 9302–9313; doi:10.1039/d2dt00416j

data_7710312
_publ_section_title
;
 High temperature spin crossover behaviour of mononuclear
 bis-(thiocyanato)iron(II) complexes with judiciously designed bidentate
 N-donor Schiff bases with varying substituents.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9302
_journal_page_last               9313
_journal_paper_doi               10.1039/d2dt00416j
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         '2(C38 H26 Cl2 Fe N6 S2)'
_chemical_formula_sum            'C76 H52 Cl4 Fe2 N12 S4'
_chemical_formula_weight         1515.03
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-01-23 deposited with the CCDC.	2022-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.7562(15)
_cell_length_b                   17.7562(15)
_cell_length_c                   12.5703(13)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    450(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.29
_cell_volume                     3963.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      450.02
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            69464
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.985
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0875 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.8514.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6346
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 717 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0810
_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^)+(0.0713P)^2^+4.2442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.2117
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2355
_reflns_number_total             3631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00416j2.cif
_cod_data_source_block           askb450_0ma
_cod_depositor_comments
'Adding full bibliography for 7710305--7710325.cif.'
_cod_original_cell_volume        3963.2(8)
_cod_database_code               7710312
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.061) H2(0.077) H3(0.082) H4(0.07) H8(0.073) H9(0.091)
 H10(0.09) H11(0.087) H12(0.074) H14(0.068) H15(0.078) H17(0.071) H18(0.059)
 Fixed X: H1(0.484739) H2(0.447439) H3(0.31967) H4(0.23198) H8(0.162821)
 H9(0.03278) H10(-0.03135) H11(0.03292) H12(0.16279) H14(0.26809) H15(0.21021)
 H17(0.1734) H18(0.22841)
 Fixed Y: H1(0.42205) H2(0.436568) H3(0.439528) H4(0.4297) H8(0.522381)
 H9(0.52702) H10(0.42599) H11(0.32227) H12(0.316429) H14(0.50787) H15(0.49229)
 H17(0.274488) H18(0.289669)
 Fixed Z: Fe1(0.5) H1(0.276039) H2(0.097301) H3(0.05576) H4(0.19683)
 H8(0.464729) H9(0.443589) H10(0.37359) H11(0.3127) H12(0.33168) H14(0.65691)
 H15(0.82569) H17(0.760241) H18(0.58906)
;
_shelx_res_checksum              54511
_olex2_submission_special_instructions 'No special instructions were received'