Effect of Intermolecular Anionic Interactions on Spin Crossover of Two Triple-Stranded Dinuclear Fe(II) Complexes Showing Above Room Temperature Spin Transition
Athira, S.; Mondal, Dibya Jyoti; Shome, Shraoshee; Dey, Bijoy; Konar, Sanjit; Dalton Transactions  (2022) –; doi:10.1039/D2DT02115C

data_7711494
_publ_section_title
;
 Effect of Intermolecular Anionic Interactions on Spin Crossover of Two
 Triple-Stranded Dinuclear Fe(II) Complexes Showing Above Room Temperature
 Spin Transition
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02115C
_journal_year                    2022
_chemical_formula_moiety         'C72 H60 Fe2 N18 O3, 4(Cl O4), 7(O), C O'
_chemical_formula_sum            'C73.35 H61.4 Cl4 Fe2 N18 O27.35'
_chemical_formula_weight         1886.10
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2022-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.903(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4510(5)
_cell_length_b                   22.6406(7)
_cell_length_c                   22.8857(8)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.23
_cell_volume                     7963.4(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1172
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            88179
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.420
_diffrn_reflns_theta_min         2.298
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5757
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1481 before and 0.0711 after correction.
The Ratio of minimum to maximum transmission is 0.7723.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             3865
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         3.484
_refine_diff_density_min         -2.117
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1144
_refine_ls_number_reflns         16294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1792
_refine_ls_R_factor_gt           0.1142
_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^)+(0.1629P)^2^+71.1216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2893
_refine_ls_wR_factor_ref         0.3357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9995
_reflns_number_total             16294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02115c2.cif
_cod_data_source_block           mo_as_82_c_0m_a
_cod_original_formula_sum        'C73.35 H61.40 Cl4 Fe2 N18 O27.35'
_cod_database_code               7711494
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Others
 Sof(Cl2A)=Sof(O8A)=Sof(O9A)=1-FVAR(1)
 Sof(Cl2)=Sof(O8)=Sof(O9)=FVAR(1)
 Fixed Sof: O11(0.5) O1AA(0.5)
3.a Free rotating group:
 O20(O22)
3.b Aromatic/amide H refined with riding coordinates:
 C56(H56), C33(H33), C32(H32), C38(H38), C57(H57), C39(H39), C9(H9), C60(H60),
 C8(H8), C52(H52), C63(H63), C36(H36), C62(H62), C35(H35), C24(H24), C18(H18),
 C12(H12), C22(H22), C59(H59), C49(H49), C23(H23), C25(H25), C41(H41), C72(H72),
  C42(H42), C17(H17), C50(H50), C66(H66), C65(H65), C69(H69), C11(H11),
 C26(H26), C28(H28), C51(H51), C1(H1), C70(H70), C4(H4), C45(H45), C21(H21),
 C46(H46), C48(H48), C71(H71), C27(H27), C2(H2), C14(H14), C47(H47), C15(H15),
 C3(H3)
3.c X=CH2 refined with riding coordinates:
 N9(H9A,H9B), N18(H18A,H18B), N7(H7A,H7B), N17(H17A,H17B), N16(H16A,H16B),
 N8(H8A,H8B)
;
_shelx_res_checksum              88170
_shelx_hkl_checksum              19178
_shelx_fab_checksum              73242
_olex2_submission_special_instructions 'No special instructions were received'