Enhanced dielectricity coupled to spin-crossover in a one-dimensional polymer iron(ii) incorporating tetrathiafulvalene.
Qiu, Ya-Ru; Cui, Long; Cai, Pei-Yu; Yu, Fei; Kurmoo, Mohamedally; Leong, Chanel F.; D'Alessandro, Deanna M; Zuo, Jing-Lin; Chemical science 11 (2020) 6229–6235; doi:10.1039/d0sc02388d

data_1558117
_publ_section_title
;
 Enhanced dielectricity coupled to spin-crossover in a one-dimensional
 polymer iron(ii) incorporating tetrathiafulvalene.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              6229
_journal_page_last               6235
_journal_paper_doi               10.1039/d0sc02388d
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         '2(C36 H34 Fe N4 O6 S6), 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C73 H70 Cl2 Fe2 N8 O12 S12'
_chemical_formula_weight         1818.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-29 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                98.637(3)
_cell_angle_beta                 99.864(3)
_cell_angle_gamma                113.651(3)
_cell_formula_units_Z            1
_cell_length_a                   11.3618(9)
_cell_length_b                   12.1577(10)
_cell_length_c                   18.2103(14)
_cell_measurement_reflns_used    3768
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      54.17
_cell_measurement_theta_min      3.71
_cell_volume                     2202.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.1066
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20722
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        51.238
_diffrn_reflns_theta_max         51.238
_diffrn_reflns_theta_min         2.208
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.191
_exptl_absorpt_correction_T_max  0.7513
_exptl_absorpt_correction_T_min  0.5516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1820 before and 0.0770 after correction.
The Ratio of minimum to maximum transmission is 0.7342.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     665
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0912P)^2^+1.1403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4591
_reflns_number_total             7221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02388d2.cif
_cod_data_source_block           complex_123k
_cod_depositor_comments
;Adding full bibliography for 1558117--1558119.cif.

 Adding full bibliography for 1558117--1558119.cif.
;
_cod_database_code               1558117
_publcif_datablock.id            {06dd0d42-84c7-48a6-bc60-1890e8396b5c}
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C28
 1.54 with sigma of 0.01
 C18-C19 = C18'-C19'
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Same fragment restrains
{S4, S2, S1, S3, C3, C4, C5, C6, C1', C2} sigma for 1-2: 0.01, 1-3: 0.04
as
{S4', S2', S1', S3', C3', C4', C5', C6, C1, C2'}
{O6, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{O6', C18', C19'}
{O6', C18', C19'} sigma for 1-2: 0.02, 1-3: 0.04
as
{O5, C27, C28}
5. Others
 Sof(O6)=1-FVAR(1)
 Sof(C18)=Sof(H18C)=Sof(H18D)=Sof(C19)=Sof(H19D)=Sof(H19E)=Sof(H19F)=0.5*(1-
 FVAR(2))
 Sof(C18')=Sof(H18A)=Sof(H18B)=Sof(C19')=Sof(H19A)=Sof(H19B)=Sof(H19C)=0.5*
 FVAR(2)
 Sof(O6')=FVAR(1)
 Sof(S2)=Sof(S1)=Sof(S4)=Sof(S3)=Sof(C2)=Sof(C5)=Sof(C4)=Sof(C1')=Sof(H1'A)=
 Sof(H1'B)=Sof(H1'C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(2)
 Sof(S4')=Sof(S2')=Sof(S1')=Sof(S3')=Sof(C3')=Sof(H3'A)=Sof(H3'B)=Sof(H3'C)=
 Sof(C4')=Sof(C5')=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2')=FVAR(2)
 Fixed Sof: Cl1(0.5) Cl2(0.5) C27(0.5) H27A(0.5) H27B(0.5) C28(0.5) H28A(0.5)
 H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5) H29B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C18'(H18A,H18B), C27(H27A,H27B), C18(H18C,H18D), C29(H29A,H29B), C25(H25A,H25B)
6.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C33(H33), C31(H31), C39(H39), C11(H11), C34(H34), C13(H13),
 C36(H36), C38(H38), C20(H20), C30(H30), C8(H8)
6.c Idealised Me refined as rotating group:
 C3'(H3'A,H3'B,H3'C), C1(H1A,H1B,H1C), C19'(H19A,H19B,H19C), C28(H28A,H28B,
 H28C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C1'(H1'A,H1'B,H1'C), C3(H3A,
 H3B,H3C), C19(H19D,H19E,H19F), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              53511
_shelx_fab_checksum              4702
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;