Spin crossover modulation in a coordination polymer with the redox-active bis-pyridyltetrathiafulvalene (py<sub>2</sub>TTF) ligand.
Zappe, Lisa; Schönfeld, Sophie; Hörner, Gerald; Zenere, Katrina A.; Leong, Chanel F.; Kepert, Cameron J.; D'Alessandro, Deanna M; Weber, Birgit; Neville, Suzanne M.; Chemical communications (Cambridge, England) 56 (2020) 10469–10472; doi:10.1039/d0cc03788e

data_7127051
_publ_section_title
;
 Spin crossover modulation in a coordination polymer with the redox-active
 bis-pyridyltetrathiafulvalene (py<sub>2</sub>TTF) ligand.
;
_journal_issue                   72
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10469
_journal_page_last               10472
_journal_paper_doi               10.1039/d0cc03788e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C34 H28 Fe N4 O4 S4, C34 H28 Fe N4 O4 S4'
_chemical_formula_sum            'C68 H56 Fe2 N8 O8 S8'
_chemical_formula_weight         1481.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2020-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-15 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                67.82(3)
_cell_angle_beta                 76.64(3)
_cell_angle_gamma                81.97(3)
_cell_formula_units_Z            2
_cell_length_a                   13.268(3)
_cell_length_b                   15.980(3)
_cell_length_c                   18.693(4)
_cell_measurement_reflns_used    5555
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      'Value not reported by XDS'
_cell_measurement_theta_min      'Value not reported by XDS'
_cell_volume                     3564.7(15)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.6897
_diffrn_measured_fraction_theta_max 0.6897
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16666
_diffrn_reflns_theta_full        31.7122
_diffrn_reflns_theta_max         31.71
_diffrn_reflns_theta_min         1.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.3774
_exptl_crystal_description       plate
_exptl_crystal_F_000             1525.9862
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.3692
_refine_diff_density_min         -0.0182
_refine_diff_density_rms         0.1823
_refine_ls_d_res_high            0.6760
_refine_ls_d_res_low             14.7720
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.1048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    142
_refine_ls_number_parameters     803
_refine_ls_number_reflns         16666
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.1022
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.1160
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1916P)^2^+16.8586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3173
_refine_ls_wR_factor_ref         0.3753
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                10878
_reflns_number_total             16666
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc03788e2.cif
_cod_data_source_block           Fepy2TTFLa
_cod_depositor_comments          'Adding full bibliography for 7127051.cif.'
_cod_original_cell_volume        3564.5(15)
_cod_database_code               7127051
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-O1 \\sim C17-O2 \\sim C67A-O5A \\sim C67B-O5B \\sim C55A-O6A \\sim C55B-O6B
 with sigma of 0.01
 C2-C1 \\sim C17-C18 \\sim C67A-C68A \\sim C67B-C68B \\sim C55A-C56A \\sim
C55B-C56B
 with sigma of 0.01
 C2-C5 \\sim C17-C15 \\sim C67A-C66A \\sim C67B-C66B \\sim C55A-C54A \\sim
C55B-C54B
 with sigma of 0.01
 C4-C5 \\sim C15-C16 \\sim C65A-C66A \\sim C65B-C66B \\sim C52A-C54A \\sim
C52B-C54B
 with sigma of 0.01
 C4-O4 \\sim C15-O3 \\sim O8A-C65A \\sim O8B-C65B \\sim C52A-O7A \\sim C52B-O7B
 with sigma of 0.01
 C4-C3 \\sim C15-C14 \\sim C64A-C65A \\sim C64B-C65B \\sim C52A-C51A \\sim
C52B-C51B
 with sigma of 0.01
 C5-C6 \\sim C16-C13 \\sim C54A-C53A \\sim C54B-C53B \\sim C66A-C63A \\sim
C66B-C63B
 with sigma of 0.01
 N2-C6 \\sim N1-C13 \\sim N7A-C53A \\sim N7B-C53B \\sim N8A-C63A \\sim N8B-C63B
 with sigma of 0.01
 N2-C7 \\sim N1-C12 \\sim N7A-C57A \\sim N7B-C57B \\sim N8A-C62A \\sim N8B-C62B
 with sigma of 0.01
 C7-C12 \\sim C57A-C62A \\sim C57B-C62B
 with sigma of 0.01
 C7-C8 \\sim C12-C11 \\sim C57A-C58A \\sim C57B-C58B \\sim C62A-C61A \\sim
C62B-C61B
 with sigma of 0.01
 C8-C9 \\sim C11-C10 \\sim C58A-C59A \\sim C61A-C60A \\sim C58B-C59B \\sim
C61B-C60B
 with sigma of 0.01
 C9-C10 \\sim C59A-C60A \\sim C59B-C60B
 with sigma of 0.01
 Fe2A-O5A \\sim Fe2A-O6A
 with sigma of 0.01
 Fe2B-O5B \\sim Fe2B-O6B
 with sigma of 0.01
3. Others
 Sof(Fe2B)=Sof(N7B)=Sof(N8B)=Sof(O5B)=Sof(O6B)=Sof(O7B)=Sof(O8B)=Sof(C51B)=
 Sof(H51a)=Sof(H51b)=Sof(H51c)=Sof(C52B)=Sof(C53B)=Sof(H53B)=Sof(C54B)=
 Sof(C55B)=Sof(C56B)=Sof(C57B)=Sof(C58B)=Sof(C59B)=Sof(H59B)=Sof(C60B)=
 Sof(H60B)=Sof(C61B)=Sof(H61B)=Sof(C62B)=Sof(C63B)=Sof(H63B)=Sof(C64B)=
 Sof(H64a)=Sof(H64b)=Sof(H64c)=Sof(C65B)=Sof(C66B)=Sof(C67B)=Sof(C68B)=
 Sof(H68a)=Sof(H68b)=Sof(H68c)=Sof(H58B)=1-FVAR(1)
 Sof(Fe2A)=Sof(N7A)=Sof(N8A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(C51A)=
 Sof(H51d)=Sof(H51e)=Sof(H51f)=Sof(C52A)=Sof(C53A)=Sof(H53A)=Sof(C54A)=
 Sof(C55A)=Sof(C56A)=Sof(C57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=
 Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(C63A)=Sof(C64A)=
 Sof(H64d)=Sof(H64e)=Sof(H64f)=Sof(C65A)=Sof(C66A)=Sof(C67A)=Sof(C68A)=
 Sof(H68d)=Sof(H68e)=Sof(H68f)=FVAR(1)
 Uiso(Fe2B)=Uiso(Fe2A)=FVAR(2)
 Uiso(N7B)=Uiso(N7A)=FVAR(3)
 Uiso(N8B)=Uiso(N8A)=FVAR(4)
 Uiso(O5B)=Uiso(O5A)=FVAR(5)
 Uiso(O7B)=Uiso(O7A)=FVAR(6)
 Uiso(O8B)=Uiso(O8A)=FVAR(7)
 Uiso(C51B)=Uiso(C51A)=FVAR(8)
 Uiso(C52B)=Uiso(C52A)=FVAR(9)
 Uiso(C53B)=Uiso(C53A)=FVAR(10)
 Uiso(C54B)=Uiso(C54A)=FVAR(11)
 Uiso(C55B)=Uiso(C55A)=FVAR(12)
 Uiso(C56B)=Uiso(C56A)=FVAR(13)
 Uiso(C57B)=Uiso(C57A)=FVAR(14)
 Uiso(C58B)=Uiso(C58A)=FVAR(15)
 Uiso(C59B)=Uiso(C59A)=FVAR(16)
 Uiso(C60B)=Uiso(C60A)=FVAR(17)
 Uiso(C61B)=Uiso(C61A)=FVAR(18)
 Uiso(C62B)=Uiso(C62A)=FVAR(19)
 Uiso(C63B)=Uiso(C63A)=FVAR(20)
 Uiso(C64B)=Uiso(C64A)=FVAR(21)
 Uiso(C65B)=Uiso(C65A)=FVAR(22)
 Uiso(C66B)=Uiso(C66A)=FVAR(23)
 Uiso(O6B)=Uiso(O6A)=FVAR(24)
 Uiso(C67B)=Uiso(C67A)=FVAR(25)
 Uiso(C68B)=Uiso(C68A)=FVAR(26)
 Fixed Sof: H63A(0.5)
 Fixed Uiso: C15(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C19(H19), C20(H20),
 C22(H22), C23(H23), C25(H25), C28(H28), C30(H30), C31(H31), C33(H33), C34(H34),
  C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C44(H44), C46(H46),
 C47(H47), C49(H49), C50(H50), C53B(H53B), C59B(H59B), C60B(H60B), C61B(H61B),
 C63B(H63B), C53A(H53A), C58A(H58A), C59A(H59A), C60A(H60A), C61A(H61A),
 C63A(H63A), C58B(H58B)
4.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C3(H3a,H3b,H3c), C14(H14a,H14b,H14c), C18(H18a,H18b,H18c),
 C51B(H51a,H51b,H51c), C64B(H64a,H64b,H64c), C68B(H68a,H68b,H68c), C51A(H51d,
 H51e,H51f), C64A(H64d,H64e,H64f), C68A(H68d,H68e,H68f)
;
_olex2_submission_special_instructions 'No special instructions were received'