Solvent-dependent SCO Behavior of Dinuclear Iron(II) Complexes with a 1,3,4-Thiadiazole Bridging Ligand.
Herold, Christian F.; Shylin, Sergii I.; Rentschler, Eva; Inorganic chemistry 55 (2016) 6414–6419; doi:10.1021/acs.inorgchem.6b00163

data_4347440
_publ_section_title
;
 Solvent-dependent SCO Behavior of Dinuclear Iron(II) Complexes with a
 1,3,4-Thiadiazole Bridging Ligand.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6414
_journal_page_last               6419
_journal_paper_doi               10.1021/acs.inorgchem.6b00163
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C32 H36 Fe2 N12 S2, 4(B F4), 4(C3 H7 N O)'
_chemical_formula_sum            'C44 H64 B4 F16 Fe2 N16 O4 S2'
_chemical_formula_weight         1404.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.733(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2504(7)
_cell_length_b                   23.3121(17)
_cell_length_c                   11.3825(6)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.904
_cell_measurement_theta_min      2.464
_cell_volume                     2979.0(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART APEX2 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2'
_diffrn_measurement_method       '\k-geometry diffractometry'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.003
_diffrn_reflns_theta_min         1.747
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker, 2008) was used for absorption correction'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_recrystallization_method 'DMF/Et2O Diffusion'
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.3909
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 4724 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.006(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         13944
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0395P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                11399
_reflns_number_total             13944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00163_si_002.cif
_cod_data_source_block           ch140
_cod_database_code               4347440
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F10A) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(F11) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(F11A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F12A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F14A) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(F15) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(F15A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(F14A)=Sof(F15A)=Sof(F16A)=1-FVAR(1)
 Sof(F14)=Sof(F15)=Sof(F16)=FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Sof(F7A)=Sof(F8A)=Sof(F6A)=1-FVAR(3)
 Sof(F6)=Sof(F7)=Sof(F8)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 N3(H3), N5(H5), N9(H9), N11(H11)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B),
 C20(H20A,H20B), C26(H26A,H26B), C27(H27A,H27B)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9A), C13(H13), C14(H14), C15(H15), C16(H16),
 C22(H22), C23(H23), C24(H24), C25(H25), C29(H29), C30(H30), C31(H31), C32(H32),
  C33(H33), C36(H36), C39(H39), C42(H42)
4.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C)
;
_shelx_res_checksum              17871
_shelx_hkl_checksum              61956
_olex2_submission_special_instructions 'No special instructions were received'