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_4347439
_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(C3 H7 N O), 4(Cl O4)'
_chemical_formula_sum            'C44 H64 Cl4 Fe2 N16 O20 S2'
_chemical_formula_weight         1454.73
_chemical_name_systematic        Fe2C44H64N16S2Cl4O20
_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                 93.887(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2852(13)
_cell_length_b                   23.666(3)
_cell_length_c                   11.4497(13)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.866
_cell_measurement_theta_min      2.453
_cell_volume                     3050.9(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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      193
_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 0.997
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31468
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.912
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.4308
_exptl_absorpt_correction_T_min  0.3520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1129 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.8171.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_recrystallization_method 'DMF/Et2O Diffusion'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.005(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         13187
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0461P)^2^+0.6200P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.837
_reflns_Friedel_fraction_max     0.804
_reflns_number_gt                11659
_reflns_number_total             13187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00163_si_003.cif
_cod_data_source_block           ch_186_0m
_cod_database_code               4347439
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.995(14) 0.005(14)
2. 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
3. Restrained distances
 O6A-O7A \\sim O6A-O8A \\sim O7A-O8A \\sim O6B-O7B \\sim O6B-O8B \\sim O7B-O8B
 with sigma of 0.02
 O5-O6A \\sim O5-O7A \\sim O5-O8A \\sim O5-O6B \\sim O5-O7B \\sim O5-O8B
 with sigma of 0.02
 Cl2-O6A \\sim Cl2-O7A \\sim Cl2-O8A \\sim Cl2-O6B \\sim Cl2-O7B \\sim Cl2-O8B
 with sigma of 0.02
 O14A-O15A \\sim O14A-O16A \\sim O15A-O16A \\sim O14B-O15B \\sim O14B-O16B
\\sim O15B-O16B
 with sigma of 0.02
 O13-O14A \\sim O13-O15A \\sim O13-O16A \\sim O13-O14B \\sim O13-O15B \\sim
O13-O16B
 with sigma of 0.02
 Cl4-O14A \\sim Cl4-O15A \\sim Cl4-O16A \\sim Cl4-O14B \\sim Cl4-O15B \\sim
Cl4-O16B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O7A) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.02
Uanis(O6B) \\sim Ueq, Uanis(O7B) \\sim Ueq, Uanis(O8B) \\sim Ueq: with sigma of
0.007 and sigma for terminal atoms of 0.02
Uanis(O14A) \\sim Ueq, Uanis(O15A) \\sim Ueq, Uanis(O16A) \\sim Ueq,
Uanis(O14B) \\sim Ueq, Uanis(O15B) \\sim Ueq, Uanis(O16B) \\sim Ueq: with sigma
of 0.007 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.02
Uanis(C43) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.02
5. Others
 Sof(O14B)=Sof(O15B)=Sof(O16B)=1-FVAR(1)
 Sof(O14A)=Sof(O15A)=Sof(O16A)=FVAR(1)
 Sof(O6B)=Sof(O7B)=Sof(O8B)=1-FVAR(2)
 Sof(O6A)=Sof(O7A)=Sof(O8A)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 N3(H3), N5(H5), N11(H11), N9(H9)
6.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)
6.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),
  C39(H39), C42(H42), C36(H36), C33(H33)
6.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              19725
_shelx_hkl_checksum              96430
_olex2_submission_special_instructions 'No special instructions were received'